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www.acs.org/acswebinars www.acs.org/acswebinars Slides available now! Recordings will be available to ACS members after one week

2016 Material Science Series “Chemistry of Hello: The Next Generation of Circuitry”


Mark Jones Executive External Strategy and

Communications Fellow, Dow Chemical

Tobin Marks Professor of Catalytic Chemistry, Materials

Science and Engineering, and Applied Physics

at Northw estern University

Co-Founder and Member of Scientif ic Advisory

Board at the Polyera Corporation

GOAL: FLEXIBLE ELECTRONIC CIRCUITRY RF ID tags, display backplanes, e-books, sensors, “smart” packaging, “smart”

displays, photovoltaics, “internet of things”

Science Needed: Versatile, Unconventional Materials

• n-Type Organic Conductors for CMOS

• Better Gate Dielectrics

• Better Understanding of Charge Transport, Interfaces

NRC/National Academies, “The Flexible Electronics Opportunity” National Academies Press, 2014

Basic Building Block: Field-Effect Transistor (FET)

12

02/02/2016

7

drain

gate / substrate

dielectric

semiconductor source

VG

VD

charge carriers

CREATES CHARGE CHANNEL IN

SEMICONDUCTOR LAYER

=> ID 0

ON VG 0

NO CHARGE CARRIERS

BETWEEN s AND d => ID = 0 OFF VG = 0

Output

plot

Transfer

plot

New Materials Must Optimize:

• Carrier mobility () & Stability

• Current on/off ratio (Ion/Ioff)

• Threshold voltage (VT)

• Subthreshold swing (SS)

• Dielectric capacitance (Ci)

Transistor Structure & Function

LCD Display Backplanes use a-Si:H

~ 0.5 cm2/V∙s-1Ion/Ioff > 106

n-type only, poor current carrier

13

Lecture Outline

I. Introduction, Challenges, Opportunities

II. New n-Type Organics

Rylenedimides

III. Nanoscopic Dielectrics

Self-Assembled Nanodielectrics

(SAND)

IV. Amorphous Oxides

Transistors

V. Conclusions, Acknowledgments

Dielectric

Semiconductor

source drain

Gate

14

02/02/2016

8

Materials Design for n-Type Semiconductors

Enablers of Organic CMOS

Molecule

Polymer

X

X R R

X

X R R

n

Substituents

Lower HOMO, LUMO

energies for electron

transport, environmental

stability

High-yield

coupling

chemistry

Substituents

Enhance solubility

Flat architecture

- stacking

Extended system to minimize

Marcus reorganization energy

Linker

Reviews: MRS Bulletin, 2010, 35, 1018; Accts. Chem. Res. 2011, 44,501; Chem. Rev. 2014, 114, 8943.

p-Type = Radical cation (h+) conductor through highest occupied MOs (HOMOs)

n-Tyep = Radical anion (e-) conductor through lowest unoccupied MOs (LUMOs)

15

Cyanoperylenes. Completely Air-Stable

n-Type Semiconductors

NN

CN

NC

O

O

O

O

RR

Crystal Structure Electrochemistry

High-yield syntheses

Good packing for efficient transport

Reduction potentials close to 0 V !(vs SCE)

Low-lying LUMO (est. -4.77 eV)

Smooth, interconnected films

AFM

1.5 1.0 0.5 0.0 -0.5 -1.0 -1.5

-1.0

-0.5

0.0

0.5

1.0

Cu

rren

t (e

-6)

Voltage

R = fluoroalkyl, alkyl, etc.

General : air stability, Ion:Ioff, Vth tunable via CN, R substituents

Suitable molecular packing, electrochemistry, film formation

Rylene review: Advanced Materials, 2011, 23, 268. 16

02/02/2016

9

Status of n-Type Molecule, Polymer Development

P-TYPE

AMBIPOLAR

AMBIPOLAR

P-TYPE

N-TYPE

AMBIPOLAR

AMBIPOLAR

N-TYPE

Best: Printable n-type air-stable polymer, μ > 2.0 cm2/Vs

Northwestern Start-up Nature 2009, 457, 679

Theoretical Guidance. Molecular Cluster, Band

Structure Approaches

n- vs. p- related to LUMO

and Homo energies

HOMO, LUMO bandwidths

comparable

Twisting from cofacial

orientation energetically

favorable, greater

bandwidths

Marcus reorganization

energies very important

M. Ratner, G. Hutchison, S. Koh, R. Ortiz, A. Freeman

Band Structure

J. Am. Chem. Soc., 2005, 127, 2339 ; 2005, 127,16866; Advan. Funct. Mater, 2008, 18, 332; J. Phys. Chem. C, 2016, submitted

t18

02/02/2016

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Inkjet-Printed Bithiophene-Imide-Based Air-Stable

Complementary Polymer Inverters

Gain ~ 40 at VDD = - 100V

Guo, X.; Ortiz, R. P.; Noh, Y.-Y.; Baeg, K.-J.; Facchetti, A.; Marks, T. J. J. Am. Chem. Soc..2015, in press. 19

20

Audience Survey Question

Which of the following statements are TRUE?

ANSWER THE QUESTION ON BLUE SCREEN IN ONE MOMENT

1. All that is needed for an organic semiconductor is a molecular π system

2. Whether an organic semiconductor is p-type or n-type is largely a function of the associated HOMO and LUMO energies

3. Electrical conductivity = mobility x carrier concentration

02/02/2016

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21




1. All that is needed for an organic semiconductor is a molecular π system

2. Whether an organic semiconductor is p-type or n-type is largely a function of the associated HOMO and LUMO energies

3. Electrical conductivity = mobility x carrier concentration

dk

Ci0

How to increase Ci :

Increase dielectric constant (κ)

Reduce thickness (d)

Ci = capacitance per area, k = dielectric constant

ε0 = vacuum permittivity, d = thickness

Parallel plate capacitor model

Need for Better Gate Dielectrics Motivates

Self-Assembled Nanodielectric (SAND)

Importance Low mobility of unconventional semiconductors

Lower operating voltages crucial for practical electronics Large densities of trapped charge → hysteresis Gate Dielectric

Functions as capacitor Stabilizes charged carriers induced by gate electric field

ISD~ VG Ci + + + + + + + + + + + +

- - - - - - - - - - - - - - - -

Typical Organic FET Data

S D

G SAND

ReviewsAdvan. Mater. 2009; Chem. Rev. 2010; Accts. Chem. Res. 2014

Dielectric Semicond.

Intel: HfO2

22 22

02/02/2016

12

SAND Gate Dielectrics Enhance Organic & Inorganic

Transistor Performance

Si Nanomembrane TFTs

Active Matrix

ZnO NW/SAND

OLED Display

Materials module deployed on the

International Space Station. Inset:

SAND-based transistors fabricated

by Northwestern scientists

Radiation-Hard SAND TFTs

Reviews: Advan. Mater. 2009, 21, 1407; Chem. Rev., 2010, 110, 205; Accts. Chem. Res. 2014

• n- and p-Type Organic Semiconductors: Molecular and Polymer

• Sorted Carbon Nanotubes, Graphene

• ZnO and In2O3 Nanowires ( μ = 3000 cm2/Vs)

• GaAs, MoS2

• Oxide Thin Films

• Conventional Si and Nanomembrane Si

23

Next-Generation SANDs Customized for Specific

Function

Type III SAND Non-Ambient Growth Hydrocarbon Solvents

Zr-SAND & Hf-SAND Ambient Growth Alcohol Solvents

V-SAND Vapor Growth Avoid Solvents

MRS Bulletin, 2010, 35, 1018; J. Am. Chem. Soc., 2011, 133, 10239; ACS Nano, 2012; Accts. Chem. Res. 2014

VA-SAND Vapor Growth Avoid Solvents

ALD Al2O3

ALD Al2O3

24

02/02/2016

13

Zr, Hf-SAND Self-Assembled Nanodielectrics

Pentacene

103

104

105

0

200

400

600

800

-3 -2 -1 0 1 2 3200

400

600

800

Capacitance (

nF

/cm

2)

Voltage (V)

Ca

pa

cita

nce

(n

F/c

m2)

f(Hz)

1 L

2 L

3 L

4 L

• Organic/inorganic hybrid multilayer

• Solution processable under ambient

• Controllable thickness, large-area uniformity, well-defined nanostructure

• High capacitance, superior insulating properties

• 350° C thermal stability

Fabrication • Self-assemble phosphonic acid-based polarizable π-molecule • Spin coat ultra-thin ZrOx primer & interlayers Organic/Inorganic TFTs

Zn-Sn-O

TEM Cross-section

Properties

M-SAND-4 (4 layer)

• Leakage: 10-7 A/cm2 @2 MV/cm

• C: 465 nF/cm2 (Zr), 1 μF/cm2

• k ≈ 11 (Zr), 20 (Hf)

• Roughness(RMS): <0.4 nm

Capacitance characteristics

Accts. Chem. Res. 2014

25

High Performance Sorted SWNT TFTs with SAND Dielectrics

Solution-Processed Z-SAND & Vapor-Deposited V-SAND

• Reduced operating voltage (2 V)

• Reduced hysteresis: reduced interfacial trapped charge; phonons?

• Higher field-effect mobility (~70 cm2/Vs) versus SiO2 dielectric (~15 cm2/Vs)

• Higher on/off ratio for same on-state conductance

SWNT Film TFT Gate Dielectric Effects

Everaerts, K.; Sangwan, V.; Jariwala, D.; Hersam, M.A.; Marks, T.J., ACS Nano 2013

VA-SAND Dielectric: µ = 150 cm2/Vs; on/off = 5 x 105, transconductance = 6.5 µS/µm

SS = 150 mV/decade

26

02/02/2016

14

Wafer-Scale SAND for Graphene Electronics

Optical micrographs of

G-FETs on Hf-SAND-4L

• Bottom contact graphene field-effect transistors (G-FETs) on 4 layers of Hf-SAND on 3” wafers

• Graphene grown by chemical vapor deposition, transferred on SAND

Sangwan, Hersam, Marks, APL, 2014, 104, 083503

• Low operating voltage (±2 V) and negligible hysteresis on Hf-SAND in vacuum

• FET = 4,500 cm2/Vs (2x higher than on Si/SiO2) (limited by quality of CVD graphene, not dielectric)

• Current saturation with intrinsic gain > 1 27

SAND Design. First-Principles Calculation of Dielectric

Response in Molecule-Based Materials

Scheme for plane-wave

DFT computation of static

dielectric response:

• Benzene Crystal: Computation: ε = 2.39; Experiment: ε = 2.34

• First powerful tool for the design of new hybrid dielectric materials

Heitzer, Marks, Ratner, JACS, 2013; JACS, 2015

ηstatic(z)

ηstatic(z) w/ substitution ηstatic(z) versus coverage

28

02/02/2016

15

Materials Design. First-Principles Calculation of Dielectric

Response in SAND-Type Materials

How to increase dielectric constant (ε) and

capacitance (C) of molecular films?

Heitzer, Marks, Ratner, ACS Nano 2014; JACS 2015.

High Surface Coverage

Low Polarizability

ε ~ 3.0

High Surface Coverage

Large Polarizability

ε > 12.0

Low Surface Coverage

Large Polarizability

ε ~ 3.0

ε = Dielectric Constant

Typical organic

films have ε ≈ 3.0,

C < 1.0 μF/cm2

Computed dielectric constant of alkane &

alkyne chains at varying surface

coverages. ε > 7.0 (C > 3.0 μF/cm2)

Computed dielectric constant of polyenes

with polarizable substituents achieve ε >

12 at 4 molecules/nm2 coverage

29

Samsung Transparent OLED TV Xconomy.com

Transparent Displays

Artefactgroup.com

Transparent Electronics Will Use Oxide TFTs + Organics

Heads-up Displays

Technology Motivation

Amorphous Oxide Driving Electronics: In-Ga-Zn-O? Can We Hybridize with Organic Materials?

Sharp IGZO Displays

30

02/02/2016

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31




1. Any polarizable substance will be a good gate dielectric for transistors

2. HfO2 is superior to SiO2 as a transistor gate dielectric because it is denser

32


Which of the following statements are TRUE? NONE


1. Any polarizable substance will be a good gate dielectric for transistors

2. HfO2 is superior to SiO2 as a transistor gate dielectric because it is denser

02/02/2016

17

Energy

np

ns

O2-: 2p6

N(ε) (DOS)

εF

ED

Metal Cation Conduction Band

• Lies above top of O-2pπ VB by ΔEgap ≥ 3.1eV

• Low enough in energy to accept electrons

• Itinerant electrons cannot be excited into higher

band by light absorption

Cation Requirements Usually Met by

• 5s CB of Cd2+, In3+, Sn4+

• Burstein-Moss increase in ΔEgap with doping

J. Goodenough

TRANSPARENT CONDUCTING OXIDE (TCO) ELECTRONIC

STRUCTURE MODEL

CB

VB

What are the Limitations and Implications of this Picture? Can We Use

These for TFTs?

PNAS 2002, JACS, 2007, MRS Bulletin, 2010, 35, 1018

Freeman, Medvedeva

Zunger

Dope to make conductive (e.g., Sn in In2O3)

33

Attractions of Amorphous Oxide Semiconductors

(AOSs) for High-Performance TFTs

• High Mobility

• Low Deposition &

Processing Temperatures

• Very Smooth Surfaces, No

Grain Boundaries

• Mechanical Flexibility

• Optical Transparency

• Properties Tunable between

Insulating, Semiconducting, Highly

Conducting by Doping

Film XRD and Electron Diffraction

Disordered Crystal Structures

Bellingham, Hosono, Fortunato, Mason, Wager 34

02/02/2016

18

Transparent a-Zn-In-Sn-O TFTs Grown by Pulsed

Laser Deposition

Transmittance ~75% (glass ~90%)

TFT Performance:

μ ~160 cm2/V·s (~20 on SiO2)

VG & VDS ~1.0 V

VT ~0.2 V

Ion:Ioff ~105

SS ~0.13 V/decade Chang, Marks Advan. Mater. 2010, 22, 2333; J. Am. Chem. Soc. 2010, 132,

11934.

Protective

Layer

35

200 300 40010

-7

10-5

10-3

10-1

101

Temp (oC)

(

cm

2/V

s)

200 300 400 50010

-1

101

103

Temp (oC)

Co

nd

uc

tiv

ity

(S

/cm

)

Low Temperature Combustion Synthesis of a-Oxide Films

Solution Precursors Oxidizer + Organic Fuel

Ignition Product

Combustion

Conventionalll

Reaction Coordinate

Ener

gy

Reaction Characterization

0

10

20

30

DT

A (V

/mg

)

200 400 600

25

50

75

100

Temp (oC)

Mass (

%)

Exo

0

20

40

60

200 400 600

25

50

75

100

Temp (oC)

Conventional Combustion

In2O3 IZO

200 300 40010

-5

10-3

10-1

101

Temp (oC)

200 300 40010

-7

10-5

10-3

10-1

101

Temp (oC)

In2O3

ZTO IZO ITO

Transistor Performance (Si/SiO2 Substrates)

TCO Conductivity

Al2O3

dielectric

Conventional Combustion

Condensed

Oxide Lattice

Kim, Fachetti, Kanatzidis, Marks Nature Materials 2011,10, 382; JACS 2016, in press. 36

02/02/2016

19

Printed a-In2O3

500 m

0.0 0.5 1.00.0

1.0

2.0

3.0

VDS

(V)

I DS (A

)

-0.5 0.0 0.5 1.01E-10

1E-9

1E-8

1E-7

1E-6

1E-5

VG (V)

I DS &

IG (

A)

VDS = 1V VG =1.00V

0.80V

0.60V

IDS

IG

Result: Inkjet Printed, Combustion-Processed Flexible

Amorphous In2O

3 Transistors on Plastic

Transistor Characterization

Research Agenda

• Materials Scope

• Microstructure Evolution

• Performance Limits, SAND

Plastic: μ = 8 cm2/V·s Ion:Ioff ~ 104

Glass: μ = 40 cm2/V·s Ion:Ioff ~105

a-Al2O3 Gate Dielectric

SAND Also Works

Kim, Fachetti, Kanatzidis, Marks Nature Materials 2011,10, 382; JACS 2015, in press. 37

Inkjet-Printed Combustion a-IGZO on Hf-SAND

SiO2 Hf-SAND-4

SiO2 Dielectric

μ ≈ 5 cm2/Vs

High operating voltage

Hf-SAND Dielectric

μMAX > 40 cm2/Vs

All-solution

processed

<3V TFT operation

Dramatic operating voltage reduction

Sputtered IGZO:

Sharp AQUOS Pad

iPad Mini Retinal Display

High mobility, no reduction in ION:IOFF 38

http://www.google.com/url?sa=i&rct=j&q=&esrc=s&frm=1&source=images&cd=&cad=rja&docid=xN9EEcGPjFDMEM&tbnid=0WosHLtavzT4GM:&ved=&url=http%3A%2F%2Fgadgetlife5.com%2Farchives%2F25546444.html&ei=EAbxUZ2QOLC4yAHKo4CwCQ&bvm=bv.49784469,d.aWc&psig=AFQjCNElX8LeadE224zHeIcLCFkOWKZSVA&ust=1374836584371334

02/02/2016

20

MRSEC -1 0 1 2 3

1E-12

1E-10

1E-8

1E-6

Cu

rre

nt

(A)

Gate Voltage (V)

Drain Current

Gate Current

Top Gated SAND/Oxide Transistors

39

Initial results are:

– µsat = 20 - 60 cm2V-1s-1

– Vth = 0.79 V

– Log (On/Off) = 7.16

Combine SAND dielectric + combustion processed IGZO

IGZO

Au

SiO2

Al Al

ITO ITO

Chang, Bedzyk, Dravid, Hersam, Marks

Fundamental Questions: • Is SAND adaptable to top gate TFTs?

• Can SAND be grown on combustion processed oxide?

• What are the characteristics of this novel interface?

Future: • Characterize microstructure, interfacial defect densities as a

function of oxide and oxide surface preparation

• Computation of interface characteristics

SA

ND

Enhanced a-TCO Performance & Low-Temp Processing

Spray-coating

Combustion

SCS

Mn+ =In3+, Ga3+, Zn2+ Oxidizer = NO3-

Fuel = Acetylacetone

M(NO3)xnH2O + Fuel MOy+ N2+H2O+CO2 + Heat

Continuous Processing: Spray Combustion Synthesis (SCS)

Bedzyk, Chang, Facchetti, Ferragut, Marks PNAS, 2015, 112, 3217

IGZO Films: Defect Density, Carrier Mobility,

Porosity ≈ Magnetron Sputtered IGZO!

40

02/02/2016

21

a-IGZO/p-SWCNT Heterojunction Electrical Properties

Rectifying diode-like output tunable with gate voltage

Anti-ambipolar transfer with two off-states and one on-state

Implications for communications keying circuitry (Mark Lundstrom)

Hersam, Lauhon, Marks, PNAS 2013, 110, 18080; NanoLett. 2015, 15, 416 41

MRSEC

In2O3 + PVP

PVP concentration

0 - 20 wt%

Chang, Bedzyk, Dravid, Marks, Advan. Mater., 2015, DOI:10.1002/adma.201405400

‘Invisible’ Flexible Transistors Enabled by Amorphous

Metal Oxide/Polymer Channel Layer Blends

Bending test for flexible TFTs

• Polymer blend with metal oxide: new route to amorphous oxide thin films

• MO:polymer blend films realize ultra flexible electronic devices

• High performance flexible transparent transistors in solution process

XRD Optical transparency

NSF-MRSEC DMR-1121262 42

02/02/2016

22

43




1. For high carrier mobilities, a regularly ordered crystal structure is essential

2. All metal oxide films are brittle, crunchy, insulating solids

3. Metal oxide transistors are used commercial in high-resolution displays

44




1. For high carrier mobilities, a regularly ordered crystal structure is essential

2. All metal oxide films are brittle, crunchy, insulating solids

3. Metal oxide transistors are used commercial in high-resolution displays

02/02/2016

23

CONCLUSIONS

Goal: Low Temperature Fabrication of Printed, Flexible, Transparent,

Unconventional Electronic Circuitry

Printable Materials for Air-Stable Organic CMOS

Design Rules for Stable n-Type Molecules, Polymers

High Performance Gate Dielectrics

Molecularly Engineered High-k SANDs for OFETs, IFETs

Low Voltage, Low Hysteresis

Hybrid Organic-Inorganic Circuitry

Organics + Inorganics: The Winner?

*Theory & Modeling Essential to Materials Design*

Understand known materials, design new ones

Applicable to Unconventional Photovoltaics

45

Northwestern University Antonio Facchetti Mark Ratner

Michael Wasielewski

Mercouri Kanatzidis

Mark Hersam

Vinayak Dravid

Mike Bedzyk

Arthur Freeman

Bob Chang

Sara Dibenedetto

Zhiming Wang

Hakan Usta

Deep Jariwala

Choongik Kim

Xinge Yu

Jeremy Smith

Rocio Ortiz

Young-Guen Ha

Lian Wang

Jun Liu

Myung-Han Yoon

Brooks Jones

Henry Heitzer

Myung-Gil Kim

Vinod Sangwan

Li Zeng

$ ONR, NSF-MRSEC, NASA, DARPA, AFOSR, $

ACKNOWLEDGMENTS

Johns Hopkins U.

Howard Katz

U. Texas Austin

Ananth Dodabalapur

U. Of Ilinois

John Rogers

Purdue U.

David Janes, Peter Ye

NASA Ames

Geetha Dholakia

U. Southern California

Chongwu Zhou

Numerous Colleagues in Europe

and Asia!

JNCASR Bangalore

K.S. Narayan, S. P. Senanayak

02/02/2016

24

Many Thanks!

47

48











02/02/2016

25

49

Thursday, March 10, 2016

Chemistry of Hello: Lithium Ion Batteries Challenges and Opportunities for Personal Electronics Applications

Dee Strand, Chief Scientific Officer, Wildcat Discovery Technologies

Mark Jones, Executive External Strategy and Communications Fellow,

Dow Chemical

2016 Material Science Series http://bit.ly/2016MaterialScienceSeries

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“Chemistry of Hello” mini-series up so just save the date!



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Chemistry of Hello: The Next Generation of Circuitry · 2016-02-04 · 02/02/2016 3 5 Let’s get Social…post, tweet, and link to ... “Chemistry of Hello: The Next Generation